Xylitol containing comestible product

ABSTRACT

The present invention relates to a process for preparing a comestible product comprising xylitol said method comprising: (a) subjecting a composition comprising xylitol in an amount ranging from about 60% to about 100% by weight to extrusion treatment inside an extrusion apparatus under conditions sufficient to form and maintain the xylitol in a slurry and (b) then shaping the extruded slurry and cooling the product to form a solid. The present invention additionally is directed to a product produced therefrom.

FIELD OF THE INVENTION

The present invention relates to a process for the production of anon-compressible comestible product comprising xylitol and thecomestible product comprising xylitol produced therefrom.

BACKGROUND OF THE INVENTION

Xylitol is a naturally occurring five carbon sugar alcohol. It occursnaturally in many fruits and vegetables and is produced by the humanbody during normal metabolism. It is a sweet crystalline product, whitein color, odorless and soluble in water. In crystalline form, it quicklydissolves in the mouth. It has a negative heat of dissolution, andthereby produces an agreeable refreshing or cooling effect in the mouth.

In addition to its cooling effect, xylitol has interesting sweeteningqualities. If one takes sucrose as a reference point, and attributes toit a sweetening value of 1, xylitol is found to have a sweetness of thesame order. Thus, xylitol is a sugar substitute. In fact, it has thesame sweetness and bulk as sucrose with one third fewer calories (2.4calories per gram) and no unpleasant after taste. It is currentlyapproved around the world for use in foods, pharmaceuticals and oralhygiene products. For example, xylitol has been widely used inconfectionery, baking products, cereals, desserts, jams, beverages,chocolate, chewing gum, gumdrops, and ice cream to name just a fewproducts. It has also been used in the production of oral hygieneproducts, such as toothpaste and in pharmaceutical products. Inaddition, it is used as a sucrose substitute placed in foods forconsumption by people with diabetes.

Further, xylitol has an interesting property for dental health, in whichit differs from other known polyols. It is, in fact, anti-cariogenic,i.e., it cannot serve as a substrate for bacteria present in the mouthcavity. Moreover, it also plays a role in preventing dental caries. Itinhibits the growth of Streptococcus Mutans, the primary bacteriaassociated with dental caries. Recent interest has increased inxylitol-containing candies because xylitol has been shown to promoteremineralization of teeth and damaged tooth enamel. It has also beenfound that regular use of xylitol can inhibit the transfer of cariogenicStreptococcus Mutans bacteria from mothers to their newborn children.Studies have shown that mothers are the primary source of infection ofStreptococcus in the mouths of newborns and that prevention or delayingcolonization by these bacteria leads to significant reduction in toothdecay later in life. In addition, xylitol reduces plaque accumulationand inhibits plaque regrowth.

Further, it also increases salivary flow. Saliva helps clean and protectteeth from decay and this plays a role in repairing the damage caused inthe early state of the decay process.

Thus, it is important to have a method of producing products comprisingxylitol for use in these various applications.

One such product is a hard candy comprised of xylitol. However,producing a hard candy of xylitol is challenging. It is difficult forxylitol to be made into a hard candy free of crystals because its glasstransition is below 32 F (0 C) and at normal household conditions, itwould exist as a liquid, although because of its instability, wouldslowly transform to a few large crystals grown loosely together.Furthermore, as a crystal, it does not compact well.

In addition, in preparing hard candies comprising xylitol, the xylitolis traditionally melted completely to form a molten mass. The moltenmass is mechanically agitated or seeded with xylitol crystals to causecrystallization. The resultant seeded mass is then combined in a layeredformat, wherein an isomalt base is first deposited, then followed by axylitol layer or the xylitol is codeposited with isomalt in a mold toproduce hard candy.

The problem often encountered in this process is that the final productis usually hygroscopic and sticky. Further, the molten mass oftenmanages to crystallize in the machinery and/or equipment, therebyclogging the machinery and/or equipment. Further, once the seed crystalshave been added, the viscosity of the seeded molten mass is verydifficult to control. Moreover, the product is very temperaturesensitive. The seeded mass thickens and crystallizes rapidly if thetemperature falls below the melting point of xylitol, and on the otherhand, thins, due to melting of the seed crystals if the temperature israised above the melting point. As a consequence, the viscosity anddensity of the seeded mass tends to vary upon prolonged exposure to amolten state which is particularly undesirable in deposited hard candymanufacturing lines where any inconsistency of the seeded mass leads toinconsistent piece weight and potential equipment failure. Further, theresultant candy is quite hard, and difficult to bite through.

The present inventors were investigating a new method for producing ahard candy comprising xylitol by modifying the methodology of the priorart. They began preparing the hard candy in a scraped surface heatexchanger, maintaining the temperature at or above the melting point ofxylitol. Even though they initially worked with a complete melt, whenthey lowered the temperature in the scraped surface heat exchanger belowthe melting point of xylitol, crystals of xylitol began to form in thescraped surface heat exchanger and begin to clog the machine. Once thexylitol recrystallized, it became extremely difficult to work with. Theinventors also noted that the product was hard and was not easily bitteninto. Moreover, the inventors have confirmed that if the temperature ofthe emitted scraped surface heat exchanger was too hot, such materialwas difficult to handle and the product obtained was undesirable.

However, the inventors found that if the xylitol was not completelymelted in an extruder, the resulting product was different and was muchsofter than the product comprising xylitol obtained from completelymelting the solid and recrystallizing the melted solid in a scrapedsurface heat exchanger. Further, in the method found by the presentinventors, since the xylitol solid was not being recrystallized, theextruder was no longer getting clogged.

The present invention thus describes this process which overcomes theproblems enumerated above and provides a product which has a high flavorimpact and a strong cooling sensation. Yet, at the same time, theproduct that is produced is a soft product that can be easily bittenthrough.

SUMMARY OF THE INVENTION

The present invention, in one embodiment, is directed to a method ofproducing a solid non-compressible comestible product comprisingxylitol, said method comprising:

-   -   (a) subjecting a composition comprising solid xylitol in an        amount ranging from about 60% up to and including 100% by weight        to extrusion treatment in an extrusion apparatus under        conditions sufficient to partially melt the xylitol in the        composition to form a slurry and maintain the composition as a        slurry as it passes through and exits the extrusion apparatus,    -   (b) forming the extruded product from step (a) into a desired        shape and    -   (c) cooling the product of(b) to form a solid.

The present invention is also directed to the product of the processdescribed hereinabove. In an embodiment, it is a comestible comprisingfrom about 60% to about 100% xylitol, having irregularly shapedcrystals, and which, when molded into a yertz shape having a base widthof 8.20 mm, a base length of 13.26 mm, a height of 8.71 mm, an angle of10% between the vertical and the side and having 0.25 mm radius filletand weighing about 0.75 grams, has a piece break pressure of less thanabout 110 MPa and a dissolution rate from about 200 to about 400seconds, said comestible having a moisture content of less than about 1%by weight of the composition, said comestible being substantially freeof monosaccharides and disaccharides and maltodextrin having a DE(dextrose equivalent) of less than 20 and sugar alcohols other thanxylitol.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 illustrates a single screw extruder system that can be utilizedin the present invention.

FIGS. 2 a, 2 b and 2 c each depict a cross section of the extrudersystem in FIG. 1.

FIG. 3 is an embodiment of a depositor.

FIG. 4 is a microscopic image magnified 400× of a drop of the xylitolcomposition in Example 10.

FIG. 5 is a photomicrograph of the drop deposited xylitol compositionfrom Example 11.

FIGS. 6 a-6 c represent photographs of a xylitol composition molded intoa yertz shape. FIG. 6 a is a front view, while FIG. 6 b is a top viewand FIG. 6 c is a side view.

DETAILED DESCRIPTION OF THE INVENTION

As described hereinabove, an embodiment of the present invention isdirected to a process of preparing a comestible product comprised ofxylitol. The comestible product within the scope of the presentinvention includes hard candies, drops, such as fruit drops or coughdrops or candy drops, and the like or any molded shaped productcomprised substantially of xylitol. Alternatively, the comestibleproduct may be a pharmaceutical. The product may be uncoated or coatedwith coatings normally used in the confectionery arts. In an embodiment,the product, including the coating, is substantially sugar free, e.g.,contains no sugar, such as sucrose. As used herein, the term “sugar”refers to aldoses and ketoses, which are monosaccharides ordisaccharides.

These sugars which are excluded include, without limit, erythrose,threose, ribose, arabinose, xylose, lyxose, allose, altrose, glucose,mannose, gulose, idose, galactose, talose, erythrulose, ribulose,xyulose, psicose, fructose, sorbose, tagatose, maltose, lactose, sucroseand the like. By being “substantially free”, it is meant that theproduct contains at most, if any, trace amounts of any sugar, i.e., thesugar content is less than about 1% by weight.

The major ingredient of the comestible product of the present inventionis xylitol. Xylitol is commercially available in a crystalline form (orgranulated form). Either form of xylitol may be used in the comestibleproduct of the present invention.

The comestible product contains at least about 60% by weight xylitol. Inone embodiment, the comestible product contains from about 60% xylitolup to and including 100% xylitol by weight and in another embodiment,from about 70% xylitol up to and including 100% xylitol by weight and ina still another embodiment from about 80% up to including 100% xylitolby weight. In another embodiment, the comestible product contains fromabout 85% xylitol to 100% xylitol by weight and in a still furtherembodiment, the comestible product contains from about 90% xylitol up toand including 100% xylitol by weight. In a still further embodiment, thecomestible product contains from about 95% xylitol up to and including100% xylitol by weight. Thus, in one embodiment, the comestible productcontains solely xylitol.

In one embodiment, the xylitol is in association with another activeproduct, e.g., a pharmaceutical. In an embodiment, the compositioncontains as much drug as possible, for example, up to and about 40% byweight drug. In an embodiment the composition comprises from about 0.01%to about 40% by weight drug, and at least about 60% xylitol by weightsuch as, for example, from about 60% to about 99.99% xylitol by weight

When xylitol is the sole active ingredient or when the comestibleproduct is a hard candy, drop or molded product, the objective is tomaximize the concentration of xylitol. In an embodiment, the xylitol ispresent in at least from about 70% by weight to about 100% by weight andin another embodiment, the xylitol is present in amount varying fromabout 80% to about 100% by weight.

Besides xylitol, the comestible product optionally contains flavorants,such as one or more food grade acids that are conventionally used inconfectionery products. In an embodiment, these flavorants are presentin flavoring effective amounts. An example of a flavorant is food gradeacid. In one embodiment, the one or more food grade acids are present inamounts ranging from about 0.01% to about 10% by weight of the product.In another embodiment, they are present in an amount ranging from about0.01% to about 5% of the product, and in still another embodiment fromabout 2% to about 4% by weight of the product.

Examples of food grade acids that may be used in the present inventioninclude, but are not limited to, malic acid, lactic acid, acetic acid,citric acid, fumaric acid, adipic acid, tartaric acid, ascorbic acid,phosphoric or salts of any of the food grade acids. The comestiblecomposition thus may comprise xylitol and optionally one food grade acidor salt thereof or a combination of one or more food grade acids orsalts thereof.

The comestible composition may optionally contain other ingredientsnormally found in confections. For example, the composition mayadditionally contain other compounds, such as vitamins, minerals orother dietary substances that have the proper stability, i.e. they arestable under the conditions for forming the comestible composition ofthe present invention. In addition, the composition may also containother flavoring agents in addition to or in lieu of the food gradeacids.

The other flavors useful in the present invention are flavors well knownfor use in comestible products, such as foods, e.g., confections. Theflavorant may be in solid form, such as a powder, crystalline, amorphouscrystal, semicrystalline and the like. They may be in the form ofliquids or they may be encapsulated or they may be spray dried. Theadditional flavors include those derived from essential oils, as well asthose flavors characterized as either natural or artificial flavors.Examples include essential oils such as, without limitation, cinnamon,spearmint, peppermint, birch, and the like; natural or artificial fruitflavors, such as, without limitation, apple, pear, peach, strawberry,cherry, apricot, orange, lemon, watermelon, banana, and the like; beanderived flavors such as, without limitation, coffee, cocoa powder andthe like. In another embodiment, the flavoring agent may be a spicecommonly used in foods. Examples include chili powder, curry powder andthe like. In another embodiment, the flavorant may be a salt commonlyused in the food arts, such as sodium chloride, potassium iodide,potassium chloride, sodium iodide and the like. In another embodiment,the comestible product of the present invention contains one or moreflavorants.

However, those flavors derived from the essence of mint oils arepreferred. In the instance where flavors, such as peppermint, spearmintand the like are prepared in accordance with the present invention, theresulting flavor composite yields a particularly cooling tastesensation. The cooling effect is attributable to the presence of xylitolin the solid crystalline form in combination with the mint oil. Thus,flavor enhancement is a further feature and benefit of the presentinvention.

As with the food grade acids, these flavoring agents are present inflavoring effective amounts. For example, they are present in amountsranging from about 0.01% to about 10% by weight and in another amountfrom about 0.01% to about 5% by weight of the composition.

In addition, another optional ingredient is a cooling agent, i.e., aningredient that imparts a cooling perception to the consumer wheningested. Examples include such agents as menthol, lemon aromas, WS 23,which is N,2,3-trimethyl-2-(1-methyl-ethyl)-butanamide, and the like.Even without the additional coolant, the comestible xylitol productdissolves quickly in the mouth and the coolness effect of the xylitol isfelt by the consumer quite quickly. The additional coolant, if present,enhances the coolness effect felt by the consumer. In an embodiment, thecooling agent is present in an amount from about 0.01% to about 2% byweight of the composition and in another embodiment from about 0.05% toabout 1% by weight if the comestible product.

However, some sugar alcohols are cooling agents. Nevertheless, thecomestible product is substantially free of sugar alcohols other thanxylitol. By substantially free, it is meant that if the comestibleproduct contains a sugar alcohol other than xylitol, then the sugaralcohol is present in such low concentrations that it does not affectany of the properties described herein, such as the dissolution rate,the break pressure point, and the like. In one embodiment, thecomestible product contains no sugar alcohol and in another embodiment,it contains trace amounts of sugar alcohol, for example, less than about2.0% by weight of sugar alcohol, and in another embodiment, the sugaralcohol is present in less than about 1.0% by weight of the product. Thecooling agents are those commercially available cooling agents normallyused in the confectionery arts, except for the sugar alcohols other thanxylitol, provided these other sugar alcohols are present in traceamounts, as described herein.

In another embodiment, the composition of the present invention issubstantially free of sugars, such as monosaccharide, disaccharide andpolysaccharide.

Cooling agents, when present, are present in an amount effective toenhance the coolness effect felt by consumers. In an embodiment, theyare present in an amount ranging from about 0.01% to about 1% by weightof the product, and in another embodiment, are present in an amountsranging from 0.01% to about 0.5% by weight of the comestible product.

There can also be added synthetic or natural food grade coloring agents,such as, for example but not limited to, azo coloring agents orcarotenoids (e.g., B carotene, canthaxathin and the like), and the like.

The total amount of these coloring agents should not exceed about 5% wtof the composition. They may be present in as low as 0.001% by weight ofthe product.

In addition, sodium bicarbonate can also be present. Its presenceeffects dissolution and provides a unique texture to the composition. Inan embodiment, when present, sodium bicarbonate reduces the density ofthe mixture. In an embodiment, the sodium bicarbonate is present in anamount effective to reduce the density of the composition relative tothe density before addition thereof. In an embodiment, sodiumbicarbonate is present in an amount ranging from about 0.01% to about10%, and in another embodiment from about 0.01% to about 5% by weight,and in another embodiment from about 0.01% to about 3% by weight of thecomestible product,

Other additional components that can be present in the comestibleproduct of the present invention include one or more food gradeprocessing agents and food additives which are typically used inconfectionery products. Examples include, but are not limited to, foodgrade preservatives, and the like. If present, they are present inamounts ranging from about 0.01% to about 5% by weight of the product.

These optional additives described hereinabove, such as food additives,e.g., food-grade acids, flavoring agents, coloring agents, food gradepreservatives, and any other components that are typically used inconfectionery products may be added as solids, or liquid form or may bepre-dried. The total amount of these optional ingredients, however, doesnot exceed about 40% by weight of the comestible product. In anotherembodiment, the total amount is no more than about 30% by weight and inanother embodiment, no more than about 20% by weight, and in a stillfurther embodiment no more than about 10% by weight of the comestibleproduct and in another embodiment, no more than about 5% by weight ofthe comestible product.

Besides candy, the comestible product may be a pharmaceutical and maycontain excipients known in the pharmaceutical arts. The pharmaceuticalmay be present in solid form, e.g., crystalline, semicrystalline oramorphous solid. The pharmaceutical may be a liquid. In addition, thexylitol in the comestible product may be present in combination with apharmaceutical such as pain-killers, e.g., aspirin, as described herein.The pharmaceutical is present in a pharmaceutically effective amount.The amount can be as low as 0.01% or 0.05% by weight and up to andincluding about 40% by weight. The pharmaceutical is present in apharmaceutically effective amount. For example, if the pharmaceutical isan analgesic, e.g., aspirin, the analgesic is present in an analgesiceffective amount. In an embodiment, the pharmaceutical is present in anamount ranging from about 0.1 to about 40% by weight. In anotherembodiment, it is present in an amount of about 5 to about 35% byweight. In another embodiment, the pharmaceutical is present in anamount ranging from about 8% to about 32% by weight. As describedhereinbelow, any pharmaceutical can be utilized as long as thepharmaceutical does not decompose under conditions, e.g., temperatureconditions, described herein in making the comestible product of thepresent invention. When a pharmaceutical is present the xylitol may bepresent from about 60% to about 99.9% by weight. In another embodiment,the xylitol may be present in at least 90% by weight and in anotherembodiment in at least 80% by weight.

The comestible product of the present invention formed by the presentprocess has a very low moisture content. In an embodiment, water ispresent in less than about 1% by weight of the comestible product. Inanother embodiment, it is present in less than about 0.5% by weight andin another embodiment, it is present in less than about 0.25% by weight.

An embodiment of the present invention is a comestible productcomprising from about 90% to about 99.9% by weight of xylitol; andoptionally from about 0.1% to about 5% by weight of one or more foodgrade acids. In another embodiment, the comestible product comprisesfrom about 95% to about 99.9% by weight of xylitol; and in anotherembodiment, the comestible product comprises xylitol in about 95% toabout 98% by weight and optionally from about 2% to about 4% by weightof one or more food grade acids.

In still another embodiment, besides the xylitol and optionally the foodgrade acid the comestible product additionally comprises a flavoringagent. In an embodiment, it additionally comprises from about 0.01% toabout 10% flavoring agent by weight. In an embodiment, the comestibleproduct comprises at least about 60% to about 100% by weight xylitol,optionally a flavoring agent, optionally cooling agent or bothoptionally flavoring agent and cooling agent. For example, in anembodiment the comestible product comprises at least about 95% xylitol,about 0.1 to about 2% flavoring agent and about 0.1 to about 0.5%cooling agent by weight.

In a further embodiment, the comestible product comprises xylitol andoptionally one or more food grade acids, as described hereinabove andoptionally a food coloring agent and a cooling agent. In a still anotherembodiment, the xylitol comestible product comprises xylitol andoptionally one or more food grade acids in the amounts as describedherein and about 0.001% to about 5% coloring agent.

In still another embodiment, the comestible product comprises xylitol,optionally one or more food grade acids and a coloring agent and aflavoring agent other than food grade acid and a cooling agent, asdescribed hereinabove.

In yet another embodiment, the comestible product of the presentinvention comprises from about 90% to about 99.9% by weight of xylitol,optionally from about 0.01% to about 5% by weight of one or more foodgrade acids, and from about 0.01% to about 3% by weight of sodiumbicarbonate. A coloring agent may additionally be present.

In an additional embodiment, the comestible product of the presentinvention comprises from about 90%, to about 99.9% by weight of xylitol,optionally from about 0.01% to about 5% by weight of one or more foodgrade acids, from about 0.01% to about 10% by weight of one or more foodgrade flavoring agents, and from about 0.01% and about 3% by weight ofsodium bicarbonate wherein the total of the additives, e.g., flavoringagents, coloring agents and sodium bicarbonate, does not exceed about20% by weight of the comestible composition.

In a still further embodiment, the comestible product of the presentinvention comprises from about 60% to and including 100% by weight ofxylitol, and optionally contains from about 0.01% to about 5% by weightof one or more food grade acids, and optionally up to about 39.99% byweight of one or more food grade processing agents and food additives.

It is to be understood, as used herein, that 100% xylitol refers to thexylitol from a very substantially pure sample (e.g., having a xylitolconcentration of greater than about 99.5% by weight) being the solecomponent. It may contain trace amounts of other components whenmanufactured, i.e., less than 0.5% by weight, but the preparation of thecomestible composition, in accordance with the procedure hereinbelowdoes not add any additional components.

The comestible product is prepared by utilizing techniques known in theart, although the actual procedure was not known heretofore. In thefirst step, the composition comprising xylitol is placed into or fedinto or passes through an extruder. If the composition contains optionalingredients, i.e., ingredients other than xylitol, a mixture comprisingthe xylitol and the other ingredient is prepared by blending the xylitolsolid and the optional ingredients, e.g., cooling agent, flavoringagent, and the like to form a substantially homogeneous mixture, i.e.,all of the ingredients are mixed thoroughly and are at leastsubstantially uniformly dispersed in the mixture. In another embodiment,the various ingredients are uniformly mixed. The components are mixed inan apparatus typically used in the art, for example, a mixer, blender,shaker or static mixer and the like.

This mixing may be effected in a mixer separate from the extruder, i.e.,it may take place prior to the mixed composition being placed into theextruder. In another embodiment, the mixing takes place within theextruder. The extruder has regions, such as a mixing zone, and thexylitol with any additional components introduced into the mixing zonefrom a feed device, e.g., feed hopper, pump and the like, is subjectedto shearing force and intense mechanical friction by the compression inthe turns of the screw. The blended xylitol composition enters theextrusion stream and is subjected to the processes describedhereinbelow.

This composition or if xylitol is the sole component, xylitol(hereinafter, the composition being drawn through in the extruder willbe referred to as the “extruder composition”) is subjected to additionalprocessing as described below. The extruder optionally contains at leastone extrusion die, although it is not necessary. Inside the extruder,there are at least one or more temperature zones which are set topredetermined temperatures. In the present process, the temperaturezones are set at temperature to partially melt the xylitol so that inthe extruder, the extruder composition is only partially melted, thatis, the xylitol is molten and contains crystalline solid. By “partiallymelted”, it is meant that the mixture is not completely melted. In otherwords, some solid material, xylitol, is maintained and not completelymelted. In accordance with the present process, seed crystals are notnecessary. In an embodiment of the present process, at least about 10%by weight of the solid is melted, while in another embodiment at leastabout 50% by weight of the solid is melted. In a still furtherembodiment, at least about 90% of the solid is melted. In a furtherembodiment, at least about 95% of the solid xylitol is melted. Asindicated hereinabove, in each of the embodiments in the presentprocess, in the extruder, not all of the solid xylitol is melted, thatis, less than 100% of the solid xylitol is melted.

It is essential that not all of the xylitol in the composition ismelted. As explained hereinbelow, the product contains crystals ofvarious sizes. Some are large and others are small. If all of thexylitol in the extruder composition is melted, then upon cooling,recrystallization will occur, creating the problems describedhereinabove, which problems are to be avoided. If the xylitolcrystallizes in the extruder, it causes the apparatus to be clogged.

The partial melting of the extruder composition in the extruder iseffected at a temperature and for sufficient amount of time so that onlya portion of the solid is melted, as described herein. In an embodiment,the temperature of the extruder composition in the extruder ranges fromabout 190 F to about 205 F and in another embodiment from about 194 toabout 200 F. The temperature at which the extruder is to be set so thatthe slurry is in this temperature range is easily determined by one ofordinary skill in the art.

By “slurry”, it is meant a translucent mass in a slushy like state. As aslurry, it contains a heterogeneous mixture of the ingredients describedhereinabove in solid and liquid form. For example, it comprises xylitolsolid mixed in with xylitol liquid and any optional ingredients. Asindicated below, the mixture remains a slurry and is not completelymelted in the extruder.

The partial melting is effected in the extruder. It can be a singlescrew extruder, a twin screw extruder or multi-screw extruder, commonlyused in the confectionery arts. The extruder may have varioustemperature zones. Generally, the various temperature zones aresufficiently high as described above, to effect the formation of theslurry and to achieve a partial melting of the xylitol therein. Theextruder composition in the extruder is at a temperature sufficientlyhigh so that the composition is partially melted but sufficiently low sothat it does not all melt. In addition, in the exit zone (also known asthe discharge zone), the temperature thereof is sufficiently high sothat the partial melt is maintained and sufficiently low so that thexylitol does not all melt. In an embodiment, the slurry in the exit zoneof the extruder is at a temperature ranging from about 190 F to about205 F, and in a still further embodiment, from about 194 F to about 200F.

In the partial melting step, the mixture is in a partial molten state,forming a slurry and remains in the slushy state. The mixture ismaintained at the appropriate temperature range at or about the meltingpoint of xylitol for a sufficient amount of time to form a slurry andmaintain the consistency of the slurry in a slushy state in and throughthe extruder and subsequent processing. If the temperature of the slurryis too low, then the slushy mixture would result in rapidcrystallization and uncontrolled hardening of the slushy mixture andpossible clogging of the equipment. If the temperature of the slurry istoo high, then more of the slush may melt and the slushy state may notbe maintained.

The slurry may be further processed to form the desired product bymethods commonly used in the confectionery industry, for example,depositing or molding. However, prior to being molded or deposited, theslurry, in one embodiment, is transferred to the depositor. Apredetermined amount of the slurry, such as in the form of a drop orsheet, is deposited onto a belt. In another embodiment, the slurry isplaced into a mold. However, prior to reaching the mold or prior to theextruded composition being deposited onto a belt, the slurry ismaintained at a temperature so that it remains a slurry. In anembodiment the slurry is maintained at or about the same temperatures aswhen present in the exit zone or as it exits from the extruder. In anembodiment, the slurry is maintained initially, after it exits theextruder at about 190 F to about 205 F and in another embodiment, about194 F to about 200 F by conventional methods known to one of ordinaryskill in the art, such as by jacketing the equipment with heating means.

In carrying out the process, the mixture in an embodiment is maintainedin a relatively dry atmosphere to prevent moisture pick up such that themoisture content does not exceed about 1% moisture.

This process of the present invention is described hereinbelow ingreater detail by referring to the drawings. The extruder contains afeeding device, for example a feed hopper or feed screw, at least oneoutlet in the discharge zone from which the extruder composition leavesthe extruder and in between, an extrusion barrel connecting the feedhopper to the outlet and which contains mixing and kneading regions andmeans of thermal regulation of the mixing and kneading regions tocontrol the temperature of the mixing regions.

An example of an extruder (12) for use in this invention is depicted inFIG. 1. It is a single screw extruder and it has a vertical feed screw(15) which forces the extrusion composition into the extrusion section(16) of the extruder (12). FIGS. 2 a, 2 b and 2 c illustratecross-sectional views of the of the extruding section of a single screwextruder (12). As depicted in FIG. 2 a, the extrusion section of asingle-screw unit is driven by a central longitudinal shaft 21 ontowhich screw segments 22 and steamlocks 23 are affixed to the shaft (SeeFIG. 2 b). The screws 22 and heating means, e.g., electric resistors orheating systems operated by induction or steam, are affixed. In FIGS. 2a, 2 b and 2 c, the heating means is a heating system operated by steam.The steamlocks 23 are arranged to provide a progressively tighter pitchand greater resistance from the inlet zone to the outlet zone. Thisarrangement results in the development of a continually increasingpressure gradient. The barrel segments 24 (FIG. 2 c) are consecutivelyaffixed onto the extruder housing and are jacketed to receive eithersteam or cooling water. These jacketed barrels assist in the developmentand control of the temperature in the extruder. Each screw segment 25 ispositioned within a corresponding barrel segment 24 to make up adesignated zone. The shaft 21 revolves at variable speeds within thebarrel to establish the required shearing conditions.

The extruder as shown can have a number of temperature zones. Theembodiment depicted in FIG. 1 has six zones in a single-screw extruder.Each zone is provided with a separate double jacket. The first zone inthe extruder 12 is the inlet zone and the last zone is the discharge orexit zone. The inlet zone contains a wide flight tapered screw designedto direct the feed mass into the barrel housing. Zones two, three, andfour desirably have screws with intermediate flight spacings intended toconvey and compress the mass. Zones five and six are equipped with“tight flight” screws. The tight flight screws work and compress themass. The discharge zone includes an exit die head. The exit die headcontains multiple hole outlets to release the extruded mass to theatmosphere.

The extrusion composition is charged into the inlet zone of the extruder12. Due to the extremely high total surface area and low moisturecontent of the extruder composition, particle-to-particle frictioncaused by the mechanical shear of the rotating screw shaft 21 generatessufficient heat to rapidly increase the temperature of the mass in theextruder barrel. If the mass is heated up too quickly, various feed-flowproblems, including the possibility of material blow-back, can occur.

In FIG. 2 zones two and three are water-cooled jackets that decrease therate of temperature rise of the extruder composition and prevent theproblems described hereinabove in the background of the invention. Evenwith these water-cooled jackets, the temperature of the extrusioncomposition in the extruder is sufficient to maintain the xylitol as aslurry, i.e., a mixture of molten xylitol and crystalline xylitol. In anembodiment, the temperature of the slurry is maintained about themelting point of xylitol. e.g., about 190 to about 205 F, while in anembodiment from about 194 to about 200 F. However, the temperature ofthe extruder is increased from friction within the extruder barrel. Theextrusion composition is kneaded in zones two and three and conveyed tozone four. In the extruder e.g., in zone four, the extruder compositionis compressed and further heated, but the extrusion composition is andremains a partial melt, a slurry. Zones four, five, and six havesteam-heated jackets that may, correspondingly, increase the amount ofliquid phase, but the extruder composition still remains a partial melt.The temperatures of zones four and five are usually controlled.

In another embodiment, the extruder is a twin-screw type extruder. Inthis embodiment, it has a feed hopper, as in the single screw extruder.It is a mixing device which kneads the mass, but instead of having onescrew, it contains a twin screw system. It may optionally have an outletdie. But it also contains a means of thermal regulation similar to thatdepicted in FIG. 1. The starting material introduced into the mixingarea is subjected to shearing forces and intense mechanical friction bythe compression in the turns of the screw and at the same time toheating which is introduced by the heating means.

The twin screw extruder has heating zones, and the temperatures of theslurry in the various zones, including the discharge zone, are asdescribed for the single screw extruder, discussed hereinabove. Again,as in the single screw extruder, the temperature of the slurry in thevarious temperature zones and in the discharge is at a temperature inwhich the xylitol forms a slurry and is maintained as a slurry. This, inone embodiment the temperature ranges from about 190 F to about 205 F,and in a further embodiment, from about 194 F to about 200 F.

Nevertheless, regardless of the type of extruder, the xylitol in thecomposition in the extruder and throughout the extruder and dischargedfrom the extruder is only partially melted. As stated above, theextruder composition is not completely melted.

Next, the slurry discharged from the extruder is formed into the desiredshape and then cooled. As described below it can any shape that isdesired. For example, it may be pastilled, deposited on a belt, molded,or sheeted to form solid product of suitable size and shape. Forexample, the slurry may be extruded from the extruder, into a depositor,as described above. The bottom of the depositor has a mechanism tocontrol the flow of materials therefrom, thus allowing it to be meteredat a desired rate. For example, the area of the depositor containspistons through which the slurry is fed and deposited onto a belt at adesired rate.

Reference is made to FIG. 3. FIG. 3 depicts the extruder discharging theslurry onto a hopper, which is part of the depositor. The depositorcontains a plurality of pistons set parallel. The pistons are arrangedso that the nozzles thereof pass through a manifold. The slurry isconveyed to the pistons.

While in the depositor, including the hopper, the partially melted slushis maintained as a partial melt. For example, it is maintained at atemperature ranging from about 190 to about 205 F and in anotherembodiment from about 194 to about 200 F. Although not shown, thedepositor, (including the hopper and the area around the pistons) isjacketed with heating means, as described above with the extruder.

The pistons work with the nozzles to assure a set amount in the form ofa drop is deposited onto the belt or into a mold Depositing the xylitolslush directly onto a belt produces a desirable rounded candy piece. Inan embodiment, it produces a rounded candy piece (sphere) when the belton which it is deposited has a contact angle above about 110° and lessthan about 180°. By contact angle, it is meant the angle at the pointwhere the outside surface of the slurry from the depositor intersects ormeets the belt. In another embodiment, the contact angle ranges fromabout 120° to about 180° and in another embodiment from about 135° toabout 1800.

The slurry discharged from the extruder may be deposited onto a belt orinto a mold to form a solid product of suitable size and shape. In anembodiment, the slurry extruded from the extruder is deposited intomolds having suitable shapes and sizes.

When placed into a mold, the slurry is cooled to a temperature where theslushy composition is a temperature at which it solidifies, e.g., it isbelow the temperature of 190 to about 205 F to allow the xylitolcontained therein to harden.

The final product from the mold or belt may be formed into a variety ofshapes that include, but are not limited to, spheres (discs),hemispheres, cubes, cuboids, pyramids, squares, rectangles, triangles,octagons, hexagons, pentagons, prisms, or a yertz, which is anelliptical cylinder which is wider at the top than at the bottom or anyother desired shape. A picture of the yertz shaped product is depictedin FIGS. 6 a-6 c. Alternatively, the final product from the mold or beltmay be formed into an irregular shape.

Once the mixture is formed into the desired shape, the formed product iscooled. This can be effected, for example, by allowing the temperatureof the slushy material to fall below the melting point of xylitol, forexample, below about 190 F. Temperatures as low as ambient temperaturesmay be used to cool the slurry to crystallize it. For example, theslurry may be passed through one or more cooling tunnels to graduallycool the formed product to room temperature. In an embodiment of thepresent invention, air is employed as a cooling medium. Air used forcooling should not be too cold to avoid sweating. In an embodiment ofthe invention, the temperature of air is between about 68 F and about104 F.

In another embodiment, air at a temperature of less than about 190 F isutilized to cool the final product. That is, the product is allowed tostand until it completely solidifies. The cooled solidified product mayoptionally be grinded to whatever size desired.

In the present process, once the temperature of the slurry is belowabout 190 F, it takes less than about ten minutes for the xylitol in thecomposition to completely solidify. In another embodiment, it takes lessthan five minutes for the xylitol in the composition to completelysolidify once the temperature is lowered to less than 190 F, while inanother embodiment it take about two to about three minutes to solidify.

The formed comestible product is then packaged. Conventional packagingmaterials and methods can be used for packaging the comestible productof the present invention based on the size and shape of the comestibleproduct.

It is to be noted that the percentage by weight of the composition ofthe present invention remains about the same throughout the process.Thus, for example, if the mixture in the first step contains about 60%xylitol, the mixture in the slurry contains xylitol at about 60% byweight and the final product contains about 60% by weight.

The moisture content throughout the process remains at about constant.More specifically, in an embodiment, the moisture content is less thanabout 1% by weight, and in another embodiment, is less than about 0.50%by weight and in a still further embodiment is less than about 0.25% byweight.

The product formed from the present process comprises at least 60%xylitol by weight. It has a low moisture content, less than about 1% byweight. Further, the dissolution rate of the product formed by thepresent process is dependent upon many factors, including the shape andweight of the product and the temperature of the solvent, usually water,in which the dissolution rate is determined. By dissolution rate, it ismeant as the time required for predetermined amount, such as 0.75 gram,to completely dissolve. Although the product may be any shape or size,for purposes of describing a characteristic of the product, a 0.75 grampiece, when molded into the shape of the yertz, as shown in FIGS. 6 a-6c, having the following dimensions: a base width of 8.20 mm, a baselength of 13.26 mm, a height of 8.71 mm, an angle of 10° between thevertical axis and the side (that is, the angle between the base and theside is 80°) and 0.25 mm radius fillet, has a break pressure point ofless than about 110 MPa. In one embodiment, the average break pressureof such a piece ranges from about 30 to about 105 MPa, and in anotherembodiment, from about 40 to about 100 M Pa. The dissolution rate ofthis sample in a 37 C bath of water ranges from about 200 seconds toabout 400 seconds, and in another embodiment from about 250 seconds toabout 350 seconds and in another embodiment, from about 290 seconds toabout 320 seconds.

The product formed from the present process is quite unique. It hasirregularly shaped crystals. It is comprised of crystals of varioussizes, wherein the size of the larger crystals is substantially largerthan the size of the smaller crystals. In an embodiment the largercrystals range from about 400 to about 600 micrometers. These varioussized crystals are randomly dispersed throughout the product. Because ofthe various crystal sizes and the looseness of the crystals in theproduct, the product of the present invention is not very hard. Thepresence of the large size crystals makes the comestible product of thepresent invention breakable without significant effort. When placed inthe mouth of the consumer, the comestible product of the presentinvention melts rapidly and the consumer feels the cooling effect andflavor more readily than if the same product was prepared byconventional methods in which the xylitol is completely melted and thenrecrystallized. Further such a product prepared by the latter method issubstantially harder than the product prepared by the present process.

In an embodiment, the comestible product of the present invention issubstantially free of any sugar alcohol other than xylitol. Examples ofthe alcohols that the comestible product is substantially free includesglycol, glycerol, erythritol, threitol, arabitol, ribitol, mannitol,sorbitol, dulcitol, iditol, isomalt, maltitol, lactitol, polydextrose,polyglycerol, and the like. It contains at most trace amounts offlavorants containing those sugar alcohols. The comestible product issubstantially free of and in an embodiment does not contain any aldosesand ketoses, including sugars, such as glucose and sucrose and contains≦2% Maltodextrin having a DE of less than 20. In another embodiment, thepresent composition is substantially free of maltodextrin, (≦1%).

The product formed is non-compressible and is preferably not a tablet,although it can be in the shape of a tablet. Therefore, no binding agentor lubricant is present in the composition. It has a crunchy texture. Bynon-compressible it is meant that the product will break into pieces ifcompressed.

The product produced may be used as a pharmaceutically active compound.As employed herein the term “pharmaceutically active compound” refers toan organic or inorganic orally ingestible compound which is taken formedicinal, dietary and nutritional purposes and which is particulate inform. As described hereinabove, xylitol has several beneficial featuresin dental hygiene. Thus, in one embodiment, the comestible product is apharmaceutical composition comprising a pharmaceutically effectiveamount of xylitol. As indicated hereinabove, in an embodiment theproduct contains at least about 80% by weight xylitol. Thepharmaceutical composition also contains excipients normally found inthe pharmaceutical arts.

Alternatively, the comestible composition comprises a pharmaceuticallyeffective amount of a pharmaceutically active compound and excipientsnormally found in the pharmaceutical arts present together with thexylitol. Many drugs, such as aspirin, when placed in the mouth dissolve,leaving a horrible taste in the mouth. By adding a pharmaceutical to thepresent composition, it is much easier to ingest because the presentcomposition masks the flavor of the pharmaceutical and makes the tastepleasant because of the cooling effect of the present composition. Anypharmaceutical may be utilized, as long as it does not decompose underthe process conditions utilized. The drugs utilized are NSAIDS, over thecounter drugs and prescribed drugs. Examples include, but are notlimited, to pain relievers, such as salicylates: aspirin (also calledacetylsalicylic acid or ASA), choline salilcylate, magnesium salicylate,and sodium salicylate and the like, acetaminophen; nonsteroidalanti-inflammatory drugs (NSAIDs: ibuprofen, naproxen sodium, andketoprofn), and the like; antihistamines, such as, loratadine,brompheniramine, chlorpheniramine, dimenhydrinate, doxylamine, and thelike; decongestants, such as pseudophedrine, phenylephrine, and thelike; laxatives, including bulk forming laxatives such asmethylcellulose, polycarbophil, psyllium, and the like; stool softenerlaxatives, such as docusate sodium and the like; saline laxatives,containing non-absorbable ions, such as magnesium, sulfate, phosphateand sodium and the like, e.g., magnesium hydroxide, magnesium citrate,sodium phosphate and the like; stimulant laxatives, such as, bisacodyl,sodium bicarbonate and potassium bitartrate, sennosides, senna, and thelike; antimetics, such as meclizine hydrochloride (Bonine),dimenhydrinate (Dramamine) and the like; oral nasal decongestants, suchas drixoral nasal decongestants and the like; cough suppressants, suchas dextromethorphan, guaifenesin, and the like; vitamins and minerals;antidiarrheal such as adsorbents, e.g., attapulgite, polycarbophil, andthe like; anti-motility antidiarrheal, such as loperamide (Imodium) andthe like; bismuth compounds, such as bismuth subsalicylate(Pepto-Bismol), and the like; drugs for treating acid ingestion, such assimethicone (Phazyme; Flatulex; Mylicon; Gas-X; Mylanta Gas), activatedcharcoal, and the like.

If an additional pharmaceutically active agent is to be present, it isprepared as described above for the comestible product. In oneembodiment, the pharmaceutical is an analgesic, e.g., aspirin. Thepharmaceutically active agent is blended with solid xylitol and with anyother pharmaceutically acceptable excipients that are normally used andthe mixture is then put into an extruder as described above. In thisembodiment, the xylitol is the pharmaceutically acceptable carrier. Asdescribed hereinabove, the xylitol in the composition is partiallymelted in the extruder. The parameters discussed above for the extruderare applicable here, including the temperature of the extrudedcomposition slurry in the discharge zone and as the slurry exits theextruder. In other words the temperature of the slurry in the exit zoneranges from about 190° F. to about 205° F. and in another embodimentfrom about 190° F. to about 200° F. Once the slurry is discharged fromthe extruder, it may be deposited, molded or pastilled. Subsequently, itis cooled and optionally milled to the desired size. The compositioncontains the medicament in effective amounts. The composition containsup to about 40% by weight of the pharmaceutically active compound and upto about 60% xylitol. For example, in an embodiment it contains aslittle as 0.01% medicament up to about 40% by weight medicament and inanother embodiment from about 1% to about 38% by weight medicament. Insuch embodiments, the amount of xylitol ranges from about 60% up toabout 99.99% xylitol and in another embodiment from about 62% up toabout 99% by weight of the composition.

Unless indicated to the contrary, the term “extruder” and “extruderapparatus” are synonymous and are used interchangeably. In addition, theexit zone of the extruder and the discharge zone of the extruder aresynonymous and are used interchangeably.

Further, unless indicated to the contrary, all percentages are by weightof the composition.

Further, the plural denotes the singular and vice versa.

In addition, the terms “slurry” and “slush” and “slushy state” are beingused interchangeability. These terms are meant to be synonymous.

Furthermore, the term “extrusion composition” refers to the compositionthat is put into the extruder.

The terms “extruder” and “extrusion apparatus”, as used herein, aresynonymous, and are being used interchangeably.

The term “substantially free”, as used herein refers to the compositionnot containing a particular component or a very small amount, but ifpresent, it does not affect any of the properties described herein. Forexample, in an embodiment, if the composition is substantially free of acomponent, refers to the component being present in less than about 2%by weight and in another embodiment less than about 1.0% and in anotherembodiment, less than about 0.1% by weight.

Unless indicated to the contrary, it is to be understood that thetemperatures are in F.

The following examples further illustrate the present invention. Theyare not meant to limit the present invention.

Example 1

Granular xylitol (98.8% w/w), powdered cooling compound WS23(N,2,3-trimethyl-2-(1-methylethyl) butanamide (0.2% w/w) and granularpeppermint flavor (1% w/w) were dry blended in a small batch mixer atambient temperature of about 65 F-75 F. The dry blending continued untila homogenous mixture was obtained. The dry blend mixture was then fedinto a water jacketed cooled hopper which feeds the product into asingle screw extruder (Wayne, Totowa, N.J. having a 24:1 L/D ratio, 1inch diameter screw in a 3:1 compression ratio). The extruder has fivetemperature controlled zones through which the mixture passed. Thetemperature in the various zones was set at about the melting point ofxylitol, and the discharge of the extruder was a 40% melted mass at 198F. The mass was solidified in a mold in the shape of mold within 2-3minutes after being placed into a mold that was then exposed to ambientair temperature. The product produced was a soft hard candy in the shapeof a mold that was easily broken by biting into it.

Example 2

Granular xylitol (98.8% w/w), powdered cooling compound WS 23 (0.2% w/w)and granular peppermint flavor (1.0% w/w) were dry blended at ambienttemperature of about 65 F-75 F. The dry blended mixture was fed into thesingle screw extruder described in Example 1. The extruder istemperature controlled in five zones, each temperature of thecomposition in each zone being about the melting point of xylitol. Thedischarge temperature of the product exiting from the extruder was about196 F. The product discharged from the extruder was about 40% melted.The product, which was a slush, was gravity drained into a heateddepositor hopper that maintained the xylitol near the melting pointrange of the xylitol, which is about 197.6-204.8 F. The product was thendeposited onto a conveyer belt where it took about 2-3 minutes tosolidify when exposed to ambient air temperature. The product is softerthan a typical hard candy.

Example 3

This example measures the dissolution rate of samples.

The following equipment was used:

-   -   1. 1000 mL Pyrex glass beakers    -   2. Octagon shaped PTFE coated 2″magnetic stir bar with molded-on        pivot ring    -   3. VWR Advanced Multiposition Stirrer—Four position stir plate        with adjustable speed controlled for all positions        simultaneously by integral knob—Catalog #12621-022    -   4. Thermometer—Mercury filled, partial immersion (76 mm        immersion), 0 C to 200 C range—calibrated against NIST traceable        digital thermometer    -   5. Three position digital timer    -   6. Deionized water    -   7. Balance, analytical—range: 0-200 gram, sensitivity+0.0001        gram    -   8. Balance, top loading electronic—range 0-3000 g.        sensitivity±0.01 gram.    -   9. Hot plate    -   10. 4 Liter Pyrex glass Erlenmeyer flask

Deionized water was heated in 4 Liter Erlenmeyer to 37 C. 600 grams ofthe heated water was divided into three separate 100 mL glass beakers.Stir bars were placed into the beakers. The beakers were positioned onthree positions of the Four position stir plate. The speed was adjustedusing digital control to 200 revolutions per minute. The watertemperature at the start and end of the dissolution procedure wasrecorded.

When a pre-weighted sample piece was dropped into each beaker, the timerwas started.

When the entire piece visibly dissolved the elapsed time was recorded asdissolution time.

The procedure was repeated each time using clean beakers and fresh 37°C. water.

The results for three samples prepared as above are depicted below:

Avg Dis- % Std Dev No. Avg % Std solution for Dissol. Measure- SampleDev for Pc Samples Rate (s) Rate ments Wt Wt Shape 1 293  6% 4 0.72371.40% yertz 2 582 7.70%   4 0.8296 7.20% yertz 3 650 12% 4 0.7505   7%yertz

The first sample (Sample 1) is the product of Example 2 described hereinabove. The second sample (Sample 2) is a sugar hard candy having a 60/40Sugar/CS ratio:

The third sample (Sample 3) is an isomalt/HSH sugar-free hard candy.

Example 4

The moisture content was measured using the Karl Fischer titrationmethod using a Brinkman Karl Fischer Titrator with homogenizer anddissolving the samples in a methanol formanide solution (3:1).

The water activity was measured as follows. Using a Instrumentation:Decagon Aqualab water activity meter connected to a computer runningAqualink Report Generator (Decagon Devices, Inc., Pullman, Wash.), thewater activity was measured as follows:

-   -   (a) Standardizing measurement: A slush of potassium chloride        crystals in distilled water is prepared such that the solution        is saturated with potassium chloride and potassium chloride        crystals are visible on the bottom of the saturated solution.        This was equilibrated to room temperature and then placed into a        small cup that was inserted into the drawer and placed into the        instrument. The reading is adjusted to be 0.859 at 15 C, 0.851        at 20 C, 0.843 at 25 C or 0.836 at 30 C (L. Greenspan. 1977. J.        Res. NBS—A. Physics and Chemistry, 81A(1):89) according to the        reported temperature.    -   (b) Sample measurement: The instrument was set to report        readings continuously.

The sample is placed into a cup placed into the instrument. The wateractivity is reported as the value which does not change by more than0.002 units between subsequent readings.

Using samples prepared in accordance with the present process describedherein, the water activity of the samples was measured as follows:

Samples Moisture Water Activity at 20 C. 4 0.24% 0.59 5 0.26% 0.50

Background for Examples 5-8 and Comparative Example 1

The procedure for measuring the texture is as follows:

Equipment:

The equipment that was used was TA.XT2i (Stable Micro Systems, Ltd.,Scarsdale, N.J.) fitted with a 30-kg measuring head with a maximum forcereading of 36800 g. Pieces were placed on a raised platform (HDP/90heavy duty platform, Stable Micro Systems, Ltd., Scarsdale, N.J.) setupon the top of the base of the instrument.

Piece shapes: The “beltDep” piece is formed in the shape of a disc(sphere) by depositing slush directly onto a room temperature belt whichprogressed through a cooling tunnel resulting in a piece with averageheight of 4.17 mm (standard deviation of 0.13-mm) and average weight of1.00-g (standard deviation of 0.036-g). The “Yertz” piece is formed bydepositing slush directly into an oval-cylinder piece with slantingsides (narrower at the bottom of the mould than the top) with a mouldbottom that was flat and 5-mm across the narrow oval axis. The mould wasscraped to remove excess slush immediately after filling beforehardening. The average height is 8.79 mm (standard deviation of 0.11 mm)and average weight of 0.746 g (standard deviation of 0.014 g). The“mouldDep” piece is formed by depositing slush directly into a mouldwith a concave bottom resulting in a piece that is flat on themould-free side and convex on the top. The average height is 5.3 mm(standard deviation of 0.66-mm) and the average weight was 1.46 g(standard deviation 0.22 g).

Fixtures

A 2 mm blunt cylinder (2 mmBlunt) (part P/2, Stable Micro Systems, Ltd,Scarsdale, N.J.) with 3.1615 mm² area; beveled blade (knife/guillotineblade of HDP/BS Blade set, Stable Micro Systems, Ltd., Scarsdale, N.J.)(bevelBlade) with 0.5-mm width of the flat area of the blade for contactwith the sample The blade contact area is 0.5 mm times the length of theblade contacting the sample.

The procedure was as follows:

0.1 mm/s to a distance or strain that results in the piece breaking,withdrawn at 10-mm/s, recording 200-pts/s. The beltDep was oriented withthe belt-side down and compressed with the 2 mm blunt probe. The yertzwas oriented with the mould-free side face-down on the platform and theprobe was placed on the flat-bottom-mould face. When using the beveledblade, the blade was oriented across the narrowest axis of the ovalwhich resulted in a contact area of 5 mm long by 0.5 mm wide or 2.5 mmarea. The mouldDep was oriented with the flat-mould-free face againstthe platform and the 2 mm-blunt probe was oriented at the apex of theconvex top.

Analysis:

maximum force at failure. The force in grams was converted to pressurein MPascals by first dividing by the area of contact and then convertingto MPascals by multiplying by 0.009807.

Software Data Collection:

Texture Exponent (Stable Micro Systems, Ltd., Scarsdale, N.J.)

Statistical Analysis:

Excel (Microsoft, Redmond, Wash.). Within a dataset, “min” and “max” arethe minimum and maximum pressure observed, respectively. “Average” isthe average value, while “median” is the 50^(th) percentile number whenranked from least to greatest. “STD dev” is the standard deviation ofthe data set and “95 CI” is the half-width of the 95% confidenceinterval for the dataset based on the standard deviation and 2-tailedt-distribution with the degrees of freedom of that dataset. “95UL” isthe estimated the upper limit for 95% of all values represented by thisdataset which is the sum of the average and 95CI.

Example 5

Xylitol with flavor was partially melted in a single screw extruder andthe slush was formed into yertz-shaped pieces that were average 8.8 mmheight and 0.75 g weight. The pieces were demoulded and tested 45 min,25 hr, 7 day and 101 days after pouring into the mould. The resultingbreak-pressures were observed.

Observed break pressure of yertz shape from slush formed on a singlescrew extruder break pressure number observed MPa 45 min 25 hr 7 day 101day <10 0% 0% 0% 0% <20 0% 0% 0% 0% <30 5% 0% 0% 0% <40 40%  12%  1% 3%<50 40%  33%  6% 10%  <60 13%  45%  30%  17%  <70 2% 11%  27%  22%  <800% 0% 17%  33%  <90 0% 0% 15%  13%  <100 0% 0% 3% 3% >100 0% 0% 0% 0%count 110 110 110 72   min, MPa 21.1 30.2 38.6 35.5 max 61.1 67.3 91.893.5 average 41.3 50.3 65.7 67.8 median 41.0 51.2 64.2 69.6 std dev 7.68.4 12.1 12.5 95CI 15.0 16.6 23.9 24.9 95UL 56.30 66.88 89.59  92.73

The data of Table I indicates that the average break-pressure does notchange after the first 7 days after forming. The data indicates that 95%of individual piece break-pressure will be less than 93-MPa after 101days. This is about 1/10^(th) of the hardness of dentine.

Example 6

Xylitol with some flavor and color was partially melted in a singlescrew extruder and the slush was fed into the hopper of a depositor,from which slush was deposited into the yertz mold. Break pressure wasdetermined on the demoulded yertz pieces 45 minutes, 1 day and 7 daysafter depositing.

Observed break pressure of xylitol-flavor slush formed in a single screwextruder, transferred to a depositor hopper and then deposited into ayertz mould peak proportion pressure observed range, MPa 45 m 1 d 1 w<20  0% <30 10% <40 33%  0% <50 43% 20%  0% <60 11% 40% 40% <70  2% 40%40% <80  1%  0%  0% <90  0% 20% >90  0% count 82   10 10 min, MPa 26.942.7 50.6 max 73.7 69.2 88.3 average 41.7 57.1 64.0 median 40.3 57.960.6 std dev  8.2 9.4 12.2 95CI 16.3 21.2 27.5 95UL 90.0 90.4 115.9

After 1 week, the average break-pressure is no different than if themould were filled with slush directly from the single screw extruder.Based on the number of observations. 95% of pieces are expected after 1week to have a break-pressure less than 116 MPa. With a larger number ofobservations as obtained in Example 1, it would be reasonable to reducethis 95UL to that of Example 5 since the standard deviation and averageare essentially the same at 1 or more weeks.

Example 7

Xylitol-flavor slush was formed using the single-screw extruder andpoured into three different moulds. The demoulded pieces were tested forbreak-pressure at ages between 7 and 27 weeks using either the 2-mmblunt probe or the beveled blade.

Comparison of xylitol pieces made from single screw extruder made indifferent shapes and anylyzed by two different probes formula xylitolxylitol xylitol xylitol xylitol shape beltDep beltDep yertz yertzmouldDep test 2 mmBlunt 2 mmBlunt 2 mmBlunt bevelBlade 2 mmBlunt age 10wk 7 wk 27 wk 27 wk 23 wk break pressure <10 MPa 0% 0% <20 MPa 6% 0% <30MPa 36%  30%   0% 0% <40 MPa 20%  30%   5% 0% 5% <50 MPa 18%  16%  15%5% 30%  <60 MPa 12%  10%  35% 0% 45%  <70 MPa 4% 6% 35% 35%  20%  <80MPa 4% 4% 10% 30%  0% <90 MPa 0% 2%  0% 25%  <100 MPa  0% 2% 5% >100MPa  0% 0% 0% count 50   50   20 20 20 min, MPa 17.2 21.0 37.9 42.8 34.4max 74.8 96.1 71.9 97.3 66.7 average 37.0 41.5 57.3 73.3 52.7 median34.5 38.4 57.9 72.1 53.1 stdev 14.6 16.7 9.3 11.2 8.0 95CI 29.3 33.619.4 23.5 16.7 95UL 66.2 75.1 76.7 96.8 69.4

The data indicate that there is some discrepancy between the 2 mm bluntprobe and the beveled blade, with the estimated 95UL being slightly lessfor the 2-mm blunt probe. The data indicate that piece shape does notaffect the 95UL break-pressure which remains under 80 MPa for the 2-mmblunt probe regardless of shape.

Example 8

A xylitol/flavor slush was formed using a twin-screw extruder andextruded into two different shapes. Each type was tested forbreak-pressure using two different fixtures. The yertz shape was testedusing the beveled blade and the molded deposit was tested using the 2-mmblunt probe.

Observed break pressure on two different shaped pieces formed by slushmade by a twin-screw extruder shape yertz discMould test bevelBlade 2mmBlunt age 1 wk 8 mo break break pressure frequency pressure MPa MPa<40 0% <40 5% <60 5% <60 25%  <80 50%  <80 65%  <100 18%  <100 5% <12023%  <115 0% <145 5% >115 0% >145 0% count 22 20 min, MPa 49.0 49.3 max144.3 82.7 average 84.8 63.2 median 78.6 62.8 std dev 23.4 12.9 95CI48.7 27.0 95UL 133.5 90.2

The data indicate that the twin-screw extruder formed pieces that had ahigher 95UL break-pressure than those formed using the single-screwextruder. The estimated 95UL break-pressure is 30 and 20 MPa higher forbeveled blade and 2-mm blunt probe fixtures, respectively.

Comparative Example 1

Hard candy both sugar and sugar-free described in Example 3 was formedinto two different mould shapes and then tested with either the beveledblade or the 2-mm blunt probe. The maximum pressure observed for thebeveled blade and 2-mm blunt probe was 144 and 115 MPa, respectively,due to the limitations of the TA.XT2i 30-kg sensing head.

Sugar or Sugar-free hard candy was formed into either the yertz ormoulded disc (discMould) and tested by two different test fixturesformula sugar sugar-free sugar shape yertz yertz discMould testbevelBlade bevelBlade 2 mmBlunt age 4 d 4 d break pressure breakpressure range, MPa proportion range, MPa <40  0%  7% <40 5% <70 13% 29%<70 0% <100 13%  7% <100 5% <130 13% 14% <115 5% >130 60% 43% >11585%  >144 47% 29% count 15 14 20 min, MPa 43 35 33 max >144 >144 >115average 118 100 109 median 138 106 115

The data indicate a very wide range of break-pressures for hard candythat encompasses values beyond the capacity of the machine. The maximumbreak-pressure was greater than 144 and 115 MPa when measuring with thebeveled blade and 2-mm blunt probe, respectively. This substantiatesthat the xylitol/flavor pieces made with the single-screw extruder havean upper limit break-pressure that is less than hard candy.

Example 9

Forming piece by depositing on a flat belt. On different samples of flatbelt was placed on 10-20 micro-liter drop of 99.5% glycerin (USP) whichis a model that behaves like the slush prepared in accordance with thepresent invention. The contact angle between the liquid drop and thebelt was measured from a back-lit 0.7-3-fold magnified photograph(Contact Angle System OCA, Data physics Instruments, GmbHRaiffeisenstraβe, Filderstadt, Germany) by using a protractor (AcmeUnited Corporation. Fairfield, Conn.). The left and right side of eachof two droplets were photographed, measured and averaged.

Belt # contact angle of glycerin drop 1 103 ± 1° 2  68 ± 1° 3  94 ± 1° 4108 ± 7° 5 143 ± 7°

The contact angle of xylitol pieces formed by depositing on differentbelt materials were backlit and photographed. The contact angle wasdetermined as the angle of its side at the point it intersects its flatbottom. Four pieces were examined measuring the contact angle on each offour points approximately at points 90° removed from each other aroundthe edge of piece.

Belt # contact angle of glycerin drop 1 90 ± 3° 2 78 ± 7° 3 106 ± 8°  4103 ± 6°  5 156 ± 15°

From this, depositing xylitol slush directly on a belt produces adesirable rounded candy piece when the belt on which it is deposited hasa contact angle about 110°.

Example 10

The drop-deposited xylitol piece of Example 2, deposited onto belt #5 ofExample 9, was examined using Contact Angle System OCA, in which thepieces were held on edge using formed aluminum foil and sidelit usingfiber-optic directed light (KL1500-Electronic, Schott North America,Inc., Elmsford, N.Y.). The images were then measured against thedistance of 1-mm also imaged under the same conditions.

The crystal sizes were identified as domains of uniform light intensitybounded completely by lighter colored lines of irregular shape. Thelongest and shortest dimensions were measured and recorded. A picture ofthe crystals is depicted in FIG. 4.

Results: Nine crystals were evident and had the following dimensions inmicrometers. 400×180, 280×280, 420×320, 580×320, 210×210, 210×210,350×140, 170×140.

Example 11

The drop-deposited xylitol piece of Example 2 was imaged along its topessentially looking along the top almost parallel to surface so as toimage the peaks and valleys. The same equipment was used as in Example10. The height of the elevations were estimated from thephotomicrographs produced, which is depicted in FIG. 5.

As shown in FIG. 5 along the top, peak to trough was observed to be lessthan 300 micrometers, while along the side near the belt, it wasobserved to be less than 50 micrometers.

Example 12

Granular xylitol (66.3% w/w), aspirin (32.5% w/w) powdered coolingcompound WS23(N. 2,3-trimethyl-2-(1-methylethyl) butanamide (0.2% w/w)and granular peppermint flavor (1% w/w) were dry blended in a smallbatch mixer at ambient temperature of about 65 F-75 F. The dry blendingcontinued until a homogenous mixture was obtained. The dry blend mixturewas then fed into a water jacketed cooled hopper which feeds the productinto a single screw extruder (Wayne, Totowa, N.J. having a 24:1 L/Dratio, 1 inch diameter screw in a 3:1 compression ratio). The extruderhas five temperature controlled zones through which the mixture passed.The temperature in the various zones was set at about the melting pointof xylitol, and the discharge of the extruder was at 198 F. The mass wassolidified in a mold in the shape of a mold within 2-3 minutes afterbeing placed into a mold that was then exposed to ambient airtemperature. The product produced was a soft hard candy in the shape ofa mold that was easily broken by biting into it.

Example 13

The process of Example 12 was repeated, except the amount of aspirinpresent was 8% (w/w) and the amount of xylitol was 91.8% (w/w).

The above preferred embodiments and examples are given to illustrate thescope and spirit of the present invention. The embodiments and theexamples described herein will make apparent to those skilled in the artother embodiment and examples. These other embodiments and examples arewithin the contemplation of the present invention.

1.-27. (canceled)
 28. A solid homogenous non-compressible comestibleproduct comprising from about 60% up to and including 100% solidxylitol, by weight and substantially free of any other sugar alcohol andsubstantially free of monosaccharides and disaccharides and maltodextrinhaving a DE of less than 20, and having a moisture content of less thanabout 1% by weight, said product, if formed into a yertz shape andhaving a base width of 8.20 mm and a length of about 13.26 mm, a heightof 8.71 mm, a 10% angle between the vertical and a side thereof andhaving 0.25 mm fillet and weighing about 0.75 grams, exhibits a piecebreak pressure of less than about 110 MPa and a dissolution rate inwater from about 200 to about 400 seconds.
 29. The comestible productaccording to claim 28 comprised of at least about 70% by weight xylitol.30. The comestible product according to claim 29 comprised of at leastabout 80% by weight xylitol.
 31. The comestible product according toclaim 30 comprised of at least about 95% by weight xylitol.
 32. Thecomestible product according to claim 28 comprising one or moreadditional ingredients selected from the flavorants, coloring agents,cooling agents, food additives and food grade processing agents.
 33. Thecomestible product according to claim 28 wherein sodium bicarbonate isadditionally present.
 34. The comestible product according to claim 31wherein sodium bicarbonate is present.
 35. The comestible productaccording to claim 28 additionally comprising a pharmaceutical.
 36. Thecomestible product according to claim 35 wherein the pharmaceutical isan analgesic.
 37. The comestible product according to claim 36 whereinthe analgesic is aspmn.
 38. The comestible product according to claim 35wherein the pharmaceutical is present in therapeutically effectiveamounts and up to about 40% by weight.
 39. The comestible productaccording to claim 38 where the pharmaceutical is present in amountsranging from about 0.01% to about 40% by weight.
 40. The comestibleproduct according to claim 28 in the form of a disc.